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題 名 | 魚肉組織中丁香酚之QuEChERs萃取及液相層析串聯質譜法檢驗方法之開發=Development of QuEChERs-based Extraction and a Liquid Chromatography-tandem Mass Spectrometry Method for Quantifying Eugenol Residues in Fish Tissues |
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作 者 | 趙偉博; 黃志能; 陳浩民; 於柏伸; 曾素香; | 書刊名 | 臺灣農業化學與食品科學 |
卷 期 | 52:2/3 2014.04-06[民103.04-06] |
頁 次 | 頁59-65 |
分類號 | 412.37 |
關鍵詞 | 魚肉組織; 超高效液相層析串聯質譜儀; 丁香酚; QuEChERs萃取; Fish tissue; Ultra high liquid chromatography/tandem mass spectrometer; Eugenol; QuEChERs extraction; |
語 文 | 中文(Chinese) |
中文摘要 | 本研究建立QuEChERs萃取方法並利用超高效液相層析串聯質譜(ultra high liquid chromatography/tandem massspectrometer, LC/MS/MS)儀之負離子電灑法,以多重反應偵測(multiple reaction monitoring, MRM)模式分析魚肉中之丁香酚。均質樣品用水分散後,加入1%醋酸之乙腈溶液配合QuEChERs萃取粉劑(硫酸鎂4 g、氯化鈉1 g、檸檬酸三鈉二水結晶鹽1 g及檸檬酸氫二鈉半水結晶鹽0.5 g)進行萃取,離心後之上清液經由primary secondaryamine、C18及無水硫酸鎂淨化,並以ACQUITY UPLC HSS T3 C18(1.8 μm, 2.1 × 100 mm)管柱搭配甲醇及去離子水做梯度流洗,再以串聯質譜儀分析,並運用基質對應檢量線(matrix-matched calibration curve)進行定量。結果顯示,於空白魚類檢體中分別添加5、10及20 ng/g濃度之丁香酚標準品,其平均回收率為99.8-107.7%之間,變異係數介於11.3-13.7%之間。本方法之定量極限為5 ng/g。 |
英文摘要 | A QuEChERs (acronym of Quick, Easy, Cheap, Effective, Rugged, and Safe) extraction method based on ultra liquid chromatography-electrospray ionization tandem mass spectrometry (LC-ESI-MS/MS) in the negative mode using multiple reaction monitoring (MRM) was developed to quantify eugenol residues in fish tissues. The homogenized sample was dispersed in water, then extracted with acetonitrile containing 1% acetic acid, and salted out with QuEChERs extraction powder (containg 4 g magnesium sulfate, 1 g sodium chloride, 1 g trisodium citrate and 0.5 g disodium citrate sesquihydrate). The supernatant obtained from high speed centrifugation, was cleaned up using a dispersive solid-phase extraction (d-SPE) with primary secondary amine, C18 and anhydrous magnesium sulfate. Analysis was performed using liquid chromatography with an ACQUITY UPLC HSS T3 C18 Column (1.8 μm, 2.1 × 100 mm) coupled to an electrospray ionization tandem mass spectrometry (LC-ESI-MS/MS) with gradient elution of methanol and water. Quantitation was performed using a matrix-matched calibration curve. Recoveries at 5, 10 and 20 ng/g spiking levels ranged from 99.8 to 107.7% and the coefficients of variation were between 11.3 to 13.7%. The quantitation limit of this method is 5 ng/g. |
本系統中英文摘要資訊取自各篇刊載內容。